JP2520493B2 - Target for forming transparent conductive film - Google Patents
Target for forming transparent conductive filmInfo
- Publication number
- JP2520493B2 JP2520493B2 JP2096256A JP9625690A JP2520493B2 JP 2520493 B2 JP2520493 B2 JP 2520493B2 JP 2096256 A JP2096256 A JP 2096256A JP 9625690 A JP9625690 A JP 9625690A JP 2520493 B2 JP2520493 B2 JP 2520493B2
- Authority
- JP
- Japan
- Prior art keywords
- target
- film
- transparent conductive
- specific resistance
- conductive film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 239000000203 mixture Substances 0.000 claims description 13
- 239000000758 substrate Substances 0.000 description 11
- 239000000843 powder Substances 0.000 description 10
- 238000002834 transmittance Methods 0.000 description 10
- 229910006404 SnO 2 Inorganic materials 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 230000007423 decrease Effects 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000005245 sintering Methods 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229910003437 indium oxide Inorganic materials 0.000 description 2
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 229910001887 tin oxide Inorganic materials 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005401 electroluminescence Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical class [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Description
本発明は透明導電膜の作成に使用するターゲットに関
する。The present invention relates to a target used for producing a transparent conductive film.
近年、情報表示機器としてフラットディスプレイが多
用されるようになり、中でも液晶表示やエレクトロルミ
ネッセンスの利用による表示が主流となってきている。
これらの表示機器は、何れも表示素子を透明導電膜で挾
みこんだサンドイッチ構造とするように構成されてい
る。 この透明導電膜は、その低い抵抗性と高い透明性とか
ら、In2O3−SnO2膜（以下、ITO膜と呼ぶ。）が最適とさ
れている。 ITO膜を得る方法としては、In2O3に、１〜10重量％の
割合となるようにSnO2を混合し、この混合物をボールミ
ルを用いて粉砕、混合し、成型・焼結し、再度ボールミ
ルを用いて粉砕し、混合し、成型・焼結することを繰返
すことにより、あるいはホットプレスを用いることによ
りターゲットを得た後、このターゲットを用いて、300
℃程度に加熱した基板上に真空蒸着あるいはスパッタリ
ングにより成膜する。このようにして得られたITO膜
は、比抵抗が2.0×10-4Ω・cm以下となることが知られ
ている。In recent years, flat displays have been widely used as information display devices, and among them, liquid crystal displays and displays using electroluminescence have become mainstream.
Each of these display devices is configured to have a sandwich structure in which a display element is sandwiched by a transparent conductive film. In this transparent conductive film, an In 2 O 3 —SnO 2 film (hereinafter referred to as an ITO film) is optimal because of its low resistance and high transparency. As a method of obtaining an ITO film, In 2 O 3 is mixed with SnO 2 in a proportion of 1 to 10% by weight, and the mixture is crushed and mixed by using a ball mill, molded and sintered, and again After crushing using a ball mill, mixing, repeating molding and sintering, or using a hot press to obtain a target, this target is used to
A film is formed by vacuum vapor deposition or sputtering on a substrate heated to about ℃. It is known that the ITO film thus obtained has a specific resistance of 2.0 × 10 −4 Ω · cm or less.
【発明が解決しようとする課題】 近年、基板として300℃のような高温に加熱できない
フィルムやコーティング樹脂上にITO膜を形成すること
が要求されてきているが、従来のターゲットを用いた場
合、200℃程度の低い基板温度で製造されたITO膜の比抵
抗が高くなり、実用的な膜が得られていない。 本発明の目的は、200℃程度の低い基板温度であって
も、蒸着あるいはスパッタリングにより充分な比抵抗を
持つITO膜を得ることを可能とさせるターゲットの提供
にある。In recent years, it has been required to form an ITO film on a film or coating resin that cannot be heated to a high temperature such as 300 ° C. as a substrate. However, when a conventional target is used, The ITO film manufactured at a low substrate temperature of about 200 ° C has a high specific resistance, and a practical film cannot be obtained. An object of the present invention is to provide a target that makes it possible to obtain an ITO film having a sufficient specific resistance by vapor deposition or sputtering even at a low substrate temperature of about 200 ° C.
本発明者らは鋭意研究を重ねた結果、用いるターゲッ
トの組成を選定すれば、基板温度を200℃程度に下げて
も、ITO膜の比抵抗が2.0×10-4Ω・cm以下となることを
見出し、本発明に至った。 すなわち、本願発明のターゲットは、（In2O3）
1-y（SnOx）ｙで示される組成を有し、ｘが1.2＜ｘ＜2.
0の範囲にあり、ｙが0.08≦ｙ≦0.20の範囲にあること
を特徴とする。As a result of intensive studies by the present inventors, if the composition of the target to be used is selected, the resistivity of the ITO film will be 2.0 × 10 −4 Ω · cm or less even if the substrate temperature is lowered to about 200 ° C. The present invention has been completed and the present invention has been achieved. That is, the target of the present invention is (In 2 O 3 )
1-y (SnO x ), having a composition represented by y , and x is 1.2 <x <2.
It is characterized in that it is in the range of 0 and y is in the range of 0.08 ≦ y ≦ 0.20.
以下、図を用いて本発明を説明する。 （In2O3）1-y（SnOx）ｙのｘとｙとを変化させて得た
ターゲットを用いて、RFマグネトロンスパッタ法によ
り、基板温度を200℃とし、ガス圧0.5Pa、導入ガスAr:O
2＝99:1、放電スパーク200W、ターゲット基板間距離40m
mとし、約3000μの膜厚になるように成膜した。 第１図は、この結果得られたITO膜の比抵抗とｘとｙ
との関係を求め、これを示したものであり、第２図は、
このITO膜の透過率とｘとｙとの関係を示したものであ
る。 第１図において、ｘ＝2.0のものは従来のものであ
り、ｙが0.08〜0.20範囲で比抵抗は2.0×10-4Ω・cmよ
り僅かに低下することがわかる。また、第１図より、ｘ
の低下により比抵抗は最初、急激に低下し、ｘがある範
囲内ではほぼ一定になり、更にｘが小さくなると、比抵
抗が急激に上昇することがわかる。これは、ｘが2.0以
上、あるいは1.0以下では、得られるITO膜中に酸素量の
欠損が生じないため、充分な導電性が発現されないから
である。 また、第２図より、ｘ＝1.0となると、透過率が急激
に低下し、実用上問題となることがわかる。これは、ｘ
＝1.2以下では、得られるITO膜中の酸素欠損が多くなり
すぎ、膜自体が金属性を帯び、光の透過性が著しく低下
し、透明導電膜としての機能を果さなくなるからであ
る。本発明において、ｘを1.2＜ｘ＜2.0の値とするの
は、上記理由からである。 第１図より、各曲線ともに、ｙが0.1のときに、比抵
抗が最小となる。各曲線がこのような挙動を示すのは、
ｙが小さすぎると、ITOの導電性の発現の原因の一つで
あるインジウムの錫による置換が効率的に行えず、結果
として低い抵抗値が得られないからであり、逆にｙが大
きすぎると、ITO膜の基本であるIn2O3結晶構造を破壊し
てしまい、低い抵抗値を得ることができなくなるからで
ある。なお、成膜時の基板温度を常温から200℃程度と
する場合、比抵抗を安定的に2.0×10-4Ω・cm以下とす
るためには、ｙは0.08≦ｙ≦0.20とすることが必要であ
る。 本発明の組成のターゲットを用いれば、基板温度が20
0℃以下であっても、充分な比抵抗を持つITO膜を形成す
ることが可能である。 本発明のターゲットを作成するに際しては、例えば、
In2O3粉末とSnO2粉末とを所定の割合で均一に混合し
て、この混合粉末を1t/cm2の圧力でプレス成形し、得ら
れた成形体を酸素濃度が10体積％以下の気流中で、1500
℃で焼結するか、あるいは酸素雰囲気中、1500℃で焼結
した後、減圧下で1200℃以上に加熱保持する。また、例
えばIn2O3粉末とSnO2粉末とSnO粉末とを所定の割合で均
一に混合し、同様に焼結処理をする。The present invention will be described below with reference to the drawings. (In 2 O 3) 1- y using a target obtained by changing the x and y (SnO x) y, by RF magnetron sputtering method, a substrate temperature of 200 ° C., gas pressure 0.5 Pa, the gas introduced Ar: O
2 = 99: 1, discharge spark 200W, target board distance 40m
The film was formed to have a thickness of m and a film thickness of about 3000 μm. Figure 1 shows the resistivity of the ITO film obtained as a result and x and y.
This is shown by seeking the relationship with
The relationship between the transmittance of this ITO film and x and y is shown. In FIG. 1, it can be seen that x = 2.0 is a conventional one and the specific resistance is slightly lower than 2.0 × 10 −4 Ω · cm when y is in the range of 0.08 to 0.20. Also, from FIG. 1, x
It can be seen that the specific resistance rapidly decreases at first due to the decrease of x, becomes almost constant within a certain range of x, and further decreases as x further increases. This is because when x is 2.0 or more, or 1.0 or less, a sufficient amount of oxygen does not occur in the obtained ITO film, and sufficient conductivity is not exhibited. Further, it can be seen from FIG. 2 that when x = 1.0, the transmittance sharply decreases, which is a practical problem. This is x
= 1.2 or less, the number of oxygen vacancies in the obtained ITO film becomes too large, the film itself becomes metallic, the light transmittance is significantly reduced, and the function as a transparent conductive film is lost. In the present invention, x is set to a value of 1.2 <x <2.0 for the above reason. From FIG. 1, in each curve, the specific resistance becomes the minimum when y is 0.1. The reason each curve shows this behavior is
This is because if y is too small, the substitution of indium with tin, which is one of the causes of the development of ITO conductivity, cannot be performed efficiently, and as a result, a low resistance value cannot be obtained. Conversely, y is too large. Then, the In 2 O 3 crystal structure that is the basis of the ITO film is destroyed, and it becomes impossible to obtain a low resistance value. When the substrate temperature during film formation is from room temperature to about 200 ° C., y should be 0.08 ≦ y ≦ 0.20 in order to stably maintain the specific resistance of 2.0 × 10 −4 Ω · cm or less. is necessary. When the target of the composition of the present invention is used, the substrate temperature is 20
Even at 0 ° C. or lower, it is possible to form an ITO film having a sufficient specific resistance. When creating the target of the present invention, for example,
In 2 O 3 powder and SnO 2 powder were uniformly mixed at a predetermined ratio, and the mixed powder was press-molded at a pressure of 1 t / cm 2 , and the resulting molded body had an oxygen concentration of 10% by volume or less. 1500 in the air
After sintering at 1500C or 1500C in an oxygen atmosphere, heat and hold at 1200C or higher under reduced pressure. In addition, for example, In 2 O 3 powder, SnO 2 powder, and SnO powder are uniformly mixed at a predetermined ratio, and the sintering process is performed in the same manner.
（実施例１） 酸化インジウム粉末と酸化錫粉末と亜酸化錫粉末との
所定量を混合して、その混合物の組成が（In2O3）４（S
nO1.5）となるようにし、ボールミルで粉砕しつつ混合
し、次いで、1t/cm2の圧力でプレス成形し、直径76mm、
厚さ5mmの円盤とし、Ar:O2＝90:10の混合気流中で５時
間、1500℃で焼結して、（In2O3）0.8（SnO1.5）0.2の
ターゲットを得た。 このターゲットを用いて、RFマグネトロンスパッタ法
により、基板温度を200℃とし、ガス圧0.5Pa、導入ガス
Ar:O2＝99:1、放電スパーク200W、ターゲット基板間距
離40mmの条件で、約3000μの膜厚のITO膜を形成した。 このITO膜における比抵抗と透過率とを測定したとこ
ろ、比抵抗が1.8×10-4Ω・cmで、透過率で85％であっ
た。 （実施例２） 酸化インジウム粉末と酸化錫粉末との所定量を混合
し、その混合物の組成が（In2O3）0.85（SnO2）0.15と
なるようにし、ボールミルで粉砕ししつつ混合し、次い
で、1t/cm2の圧力でプレス成形し、直径76mm、厚さ5mm
の円盤を作成し、この円盤をAr:O2＝90:10の混合気流中
で５時間、1500℃で焼結させ、（In2O3）0.85（Sn
O1.9）0.15のターゲットを得た。 このターゲットを用いて実施例−１と同様にしてITO
膜を形成し、比抵抗と透過率とを測定したところ、比抵
抗は1.9×10-4Ω・cmであり、透過率は86％であった。 （実施例３） 実施例−２と同様にして、直径76mm、厚さ5mmの円盤
を作成し、この円盤を酸素気流中1500℃で５時間焼結
し、次いで、真空中で1200℃に１時間保持して、（In2O
3）0.85（SnO1.7）0.15のターゲットを得た。 このターゲットを用いて前記実施例と同様にしてITO
膜を形成し、比抵抗と透過率とを測定したところ、比抵
抗は1.9×10-4Ω・cmであり、透過率87％であった。Example 1 A predetermined amount of indium oxide powder, tin oxide powder, and tin suboxide powder was mixed, and the composition of the mixture was (In 2 O 3 ) 4 (S
nO 1.5 ), pulverize and mix with a ball mill, then press-mold at a pressure of 1 t / cm 2 to obtain a diameter of 76 mm,
A disk having a thickness of 5 mm was used and sintered at 1500 ° C. for 5 hours in a mixed air stream of Ar: O 2 = 90: 10 to obtain a target of (In 2 O 3 ) 0.8 (SnO 1.5 ) 0.2 . Using this target, the substrate temperature was set to 200 ° C by the RF magnetron sputtering method, the gas pressure was 0.5 Pa, and the introduced gas was
An ITO film having a thickness of about 3000 μm was formed under the conditions of Ar: O 2 = 99: 1, discharge spark 200 W, and a distance between target substrates of 40 mm. When the specific resistance and the transmittance of this ITO film were measured, the specific resistance was 1.8 × 10 −4 Ω · cm and the transmittance was 85%. (Example 2) A predetermined amount of indium oxide powder and tin oxide powder was mixed so that the composition of the mixture was (In 2 O 3 ) 0.85 (SnO 2 ) 0.15, and the mixture was pulverized with a ball mill and mixed. , Then press-molded with a pressure of 1t / cm 2 , diameter 76mm, thickness 5mm
Disk was prepared, and this disk was sintered at 1500 ° C for 5 hours in a mixed air flow of Ar: O 2 = 90: 10, and then (In 2 O 3 ) 0.85 (Sn
O 1.9 ) 0.15 target was obtained. Using this target in the same manner as in Example-1, ITO
When a film was formed and the specific resistance and the transmittance were measured, the specific resistance was 1.9 × 10 −4 Ω · cm, and the transmittance was 86%. (Example 3) A disk having a diameter of 76 mm and a thickness of 5 mm was prepared in the same manner as in Example-2, and the disk was sintered in an oxygen stream at 1500 ° C for 5 hours, and then in vacuum at 1200 ° C. Hold the time, (In 2 O
3 ) A target of 0.85 (SnO 1.7 ) 0.15 was obtained. This target is used to perform ITO in the same manner as in the above embodiment.
When a film was formed and the specific resistance and the transmittance were measured, the specific resistance was 1.9 × 10 −4 Ω · cm, and the transmittance was 87%.
本発明のターゲットを用いれば、基板温度が200℃以
下であっても比抵抗が2.0×10-4Ω・cm以下の良好なITO
膜が得られる。 したがって、従来技術より約100℃以上も低い温度でI
TO膜の作製が可能となり、許容温度の低いフィルムやコ
ーティング樹脂へITO膜作製の適用範囲が拡がるる。When the target of the present invention is used, a good ITO having a specific resistance of 2.0 × 10 −4 Ω · cm or less even if the substrate temperature is 200 ° C. or less
A film is obtained. Therefore, I
The TO film can be manufactured, and the application range of the ITO film can be extended to films and coating resins with low allowable temperatures.
第１図は、本発明の実施例にかかるターゲットを用いて
作成したITO膜の比抵抗とターゲットの組成との関係を
示したグラフ。 第２図は、第１図のITO膜の透過率とターゲットの組成
との関係を示したグラフ。FIG. 1 is a graph showing the relationship between the resistivity of an ITO film formed using the target according to the example of the present invention and the composition of the target. FIG. 2 is a graph showing the relationship between the transmittance of the ITO film of FIG. 1 and the composition of the target.
Claims (1)
有し、ｘが1.2＜ｘ＜2.0の範囲にあり、ｙが0.08≦ｙ≦
0.20の範囲にあることを特徴とする透明導電膜形成用タ
ーゲット。1. A composition represented by (In 2 O 3 ) 1-y (SnO x ) y , x is in the range of 1.2 <x <2.0, and y is 0.08 ≦ y ≦.
A target for forming a transparent conductive film, which is in the range of 0.20.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2096256A JP2520493B2 (en) | 1990-04-13 | 1990-04-13 | Target for forming transparent conductive film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2096256A JP2520493B2 (en) | 1990-04-13 | 1990-04-13 | Target for forming transparent conductive film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03295114A JPH03295114A (en) | 1991-12-26 |
| JP2520493B2 true JP2520493B2 (en) | 1996-07-31 |
Family
ID=14160119
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2096256A Expired - Lifetime JP2520493B2 (en) | 1990-04-13 | 1990-04-13 | Target for forming transparent conductive film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2520493B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4413344A1 (en) * | 1994-04-18 | 1995-10-19 | Leybold Materials Gmbh | Process for the production of partially reduced indium oxide-tin oxide targets |
| WO2001045182A1 (en) * | 1999-12-17 | 2001-06-21 | Institute Of Materials Research & Engineering | Improved transparent electrode material for quality enhancement of oled devices |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS54136224A (en) * | 1978-04-14 | 1979-10-23 | Matsushita Electronics Corp | Target electrode for color pick up tube and its manufacture |
| JPS55131902A (en) * | 1979-04-02 | 1980-10-14 | Mitsubishi Electric Corp | Method of fabricating transparent conductive film |
-
1990
- 1990-04-13 JP JP2096256A patent/JP2520493B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH03295114A (en) | 1991-12-26 |
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